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500 个结果
  • 简介:TheepoxidationofallylchloridewithH2O2onTi-ZSM-5preparedbyisomorphoussubstitutionofHZSM-5withTiCl4gaswasstudied.TheresultsshowthatTi-ZSM-5hasahighcatalyticefficiencyfortheepoxidationofallylchloride.TheH2O2utilizationreaches99.50%whentheallylchloride/H2O2molarratiois>1.Theeffectofsolventspecies,catalystconcentration,H2O2andallylchlorideconcentrationandreactiontemperatureontheepoxidationwasinvestigatedsimultaneously.Itisfoundthatmethanolisthebestsolventforthereaction.Thereactionrateequationwithv=k[Cat.][H2O2]1/2-[C3H5Cl]andtheapparentactivationenergywithEa=63.462kJ/molareobtainedaccordingtothekineticsstudy.

  • 标签: TI-ZSM-5 EPOXIDATION of ALLYL chloride epichloro-hydrin
  • 简介:TheternaryCu(Ⅱ)complexwith2,2′-bipyridyl(bipy)andL-methioninte(L-Met)hasbeensynthesizedandcharacterizedbyelementalanalysis,molarconductivity,UV-Visspectra,IRspectraandpH-potentiometrictitrationmethods.Thestructureofthecomplex[Cu(L-Met)(bipy)(H2O)]ClO4·3/8H2OwascharacterizedbytheX-raydiffractionanalysis.Itcrystallizesinthetriclinicsystem,spacegroupP1withfourmoleculesinaunitcellofdimensions,a=0.7656(2)nm,b=1.3142(3)nm,c=2.0596(4)nm,α=97.70(3)°,β=97.96(3)°,γ=94.33(3)°,V=2.0244(8)nm^3,R1=0.0441andwR2=0.0678,Thecrystalcontainsfourcrystallographicallyindependent[Cu(L-Met)(bipy)(H2O)]^+complexes(Cu1-Cu4),havingadistortedsquare-pyramidalgeometrywiththesamecoordinatedatomsaroundeachcoppercenter.Thebaseplaneisoccupiedbytwonitrogenatomsofonebipy,theaminonitrogenatomandonecarboxylateoxygenatomfromeachindependentL-Metmoiety,andonewateroxygenatanaxialposition.CulandCu3areessentiallyenantiomersofCu2andCu4.Thefourmoleculesarepackedwitheachotherbyintermolecularhydrogen-bondingandaromatic-ringstackinginteractions.

  • 标签: 铜(Ⅱ)配合物 2 2′-二吡啶 L-蛋氨酸 合成 分子结构 表征
  • 简介:Variousenolsof2-acylmethyl-4,4-dimethyl-2-oxazolineswerepreparedinmoderateyieldsviaultrasonicallycatalyzedreactionsof2,4,4-trimethyl-2-oxazolinewitharenecarboxylicestersinthepresenceofUDP-t-BuCl-i-Pr2NHsystem.

  • 标签: Ultrasonically dispersed POTASSIUM 2 4 4-trimethyloxazoline
  • 简介:Thepaperdealswiththeinfluenceofanodematerialontheefficiencyofdegradationfororganicpollutantsinwatersystem.Theelectrochemicalperformanceoffluorineiondopedleaddioxide(F--PbO2)electrodeforthedegradationofanilinewascomparedwiththatofundopedleaddioxide(PbO2)electrodebyultraviolet-visible(UV-Vis)spectroscopy,linearvoltammetryandotheranalyticalmethods,suchasthemeasurementbychemicaloxygendemandanalyzer,highperformanceliquidchromatographyandscanningelectronmicrography.ItwasshownthatbothPbO2electrodeandF--PbO2electrodecouldmakeanilinebemineralizedcompletelyandhavethesamedegradationcourse,butF--PbO2electrodehasmuchhigherelectrocatalyticactivitythanundopedPbO2electrodefortheelectrochemicaldegradationofaniline.TheexperimentalresultsconfirmthatF--PbO2electrodehasmuchhigherpotentialforoxygenevolutionthanundopedPbO2electrode.

  • 标签: 二氧化铅阳极 电化学降解 电化学性能 掺杂 苯胺 PBO2电极
  • 简介:Tris)(η5-cyclopentadienyl-μ-carbonyl-iron)-μ3-nitrosylclusterwasobtainedfromthereactionofcyclopentadienyldicarbonylirondimerwithnitrogenmonoxideinxylene.Theclusterwascharacterizedbyelementalanalyses,IR,MSand1HNMR.Thecrystalstructureof[(η5-C5H5)(μ-CO)Fe]33-NO).C4H8OwasdeterminedbyX-raydiffractionanalysis.ItcrystallizesintheorthorhombicspacegroupPnma,a=9.053(2),6=10.545(2),c=22.525(4)A,V=2150.3(7)A3,Z=4,Dc=1.68g.cm-3;structuresolutionandrefinementbasedon1141reflectionswithI>3.0(I)(MoKa,A=0.71073A)convergedatR=0.0540.Theinfraredabsorptionbandat1325cm-1oftheμ3-NOinthecluster,whichisredshifted,showsthatμ3-NOisactivated.

  • 标签: NITROSYL complexes iron CLUSTER NO activation.
  • 简介:Anovelsupportedliquidphasefilmcatalyst:SupportedPdCl2-(n-C4H9)4N+Cl-moltensaltswasfoundtobeaneffectivecatalystwithgoodstabilityforselectivehydrodechlorinationofCCl2F2(CFC-12)toitsalternativesCH2F2andCHClF2.AdditionofCoCl2,GaCl3andCuCl2toPdCl2-(n-C4H9)4N+Cl-modifiesthecatalyticperformanceofsupportedmoltensalts.

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  • 简介:传统的化学分析方法分析硅酸盐类矿物样品组份,操作过程繁琐、分析周期长、劳动强度较大,分析结果受分析人员及各种试剂因素影响较大。采用国产能量色散X-射线荧光分析仪,以Li2B4O7和LiBO2作混合熔剂,NH4NO3为氧化剂,熔融制作玻璃熔片,对硅酸盐中SiO2等10个主要成分含量进行同时分析,建立了能量色散X-射线荧光光谱法测定硅酸盐主成分含量的方法,准确度和精密度均达到了规范要求,得到了较为满意的分析结果。

  • 标签: 能量色散X-射线荧光光谱法 硅酸盐 主成分
  • 简介:铷矿石和混合熔剂按照一定的质量比混配好,在熔样机中制备成待分析的样品,混合熔剂由四硼酸锂'偏硼酸锂'氟化锂按照一定比例混合而成,通过对国家标准物质不同质量的稀释或者在其中添加纯物质的办法制备成一系列的含不同氧化铷的标准系列样片,采用X射线荧光光谱仪直接测定氧化铷的含量。方法的测定范围0.01%~5.0%,相对标准偏差(RSD)小于1.5%,同时对标准样品的种类要求少,而通过某一标准物质来制备校正曲线也可以克服基体效应的影响。方法适应于稀有矿石类标准物质数量和种类矿石不多的分析,对国家一级标准物质分析准确度高。

  • 标签: 铷矿石 混合熔剂 质量稀释 熔融法 X射线荧光光谱法
  • 简介:针对多种类不锈钢多元素成分解析问题,应用X射线荧光光谱分析软件UniQuant,采用扩展基本参数法对多元不锈钢、双相不锈钢进行光谱干扰校正和基体校正,重新设定和优化多元不锈钢基体元素的测试条件,计算背景因子、杂质因子、谱线灵敏度系数和光谱重叠系数,测定Si、Mn、S、P、Ni、Cr、Cu、Mo、V、Al、Ti、Nb、Co、Ta、Fe的相对标准偏差在0.04%-3.8%,Ca、Zr、W、As、Sb、Sn的相对标准偏差在5.4%-20.3%,未知样品检测值与认定值比对结果相当理想,Ni、Cr的平均偏差小于0.05%,可以用很少标准样品实现各类型不锈钢多元素成分准确检测,检测范围宽,适用性好。

  • 标签: X射线荧光光谱法 扩展基本参数法 不锈钢
  • 简介:提出了以自制的标准样品,采用单点法绘制校准曲线,利用X射线荧光光谱仪测定FeSiB非晶薄带样品中硅、硼和铁的含量。对于4个FeSiB非晶合金薄带样品中硅、硼和铁进行了10次测定,其分析结果的相对标准偏差分别为0.4%~0.5%、1.3%~4.2%和0.2%~0.4%。方法的分析结果与火花源原子发射光谱法、化学重量法和电感耦合等离子体原子发射光谱(ICP-AES)法的测定值吻合较好。方法快速、简便,薄带样品无需制样,适用于FeSiB非晶合金薄带的快速成分分析。

  • 标签: X射线荧光光谱法(XRF) FeSiB非晶合金薄带 FeSiB合金 单点法
  • 简介:合成了N,N′-亚水杨基皮考林酰肼(HL)及其铁配合物[FeL2](C26H20FeN6O4,Mr=536.33).X射线衍射实验结果表明,标题配合物晶体属于正交晶系,空间群为Pbcn,晶体学参数:a=1.4970(1)nm,b=1.51556(9)nm,c=2.0920(2)nm,V=4.7462(6)nm3,Z=8,Dc=1.501Mg·m-3,F(000)=2208,μ(MoKα)=0.682mm-1,R=0.0695,Rw=0.1502.在配合物[FeL2]中,铁(Ⅱ)原子具有扭曲的八面体配位构型,晶体通过分子间氢键作用形成缔合分子对.红外光谱表明,配体在形成配合物后,ν(CO)和ν(CN)红移.电子光谱表明存在π-π*和d-π*的跃迁;荧光光谱表明,配合物金属对配体n-π*激发引起的荧光发射峰有较大的影响.

  • 标签: N N′-亚水杨基皮考林酰肼 铁配合物 晶体结构 荧光性质 氢键
  • 简介:TheelectrochemicalbehaviorsandthedetectionofNO2-haveattractedincreasingattentionrecentlybecauseoftheimportantrolesplayedbyNO2-inenvironmentandlifeprocesses.Thus,advancedtechniquesforthedetermination,especiallyon-sitedetermination,ofthenitriteinfoods...

  • 标签: NITRITE REDUCTION MICROELECTRODE CE mechanism
  • 简介:TwonewcoenzymeB12analogues,2’,5’-dideoxycytidylcobalamin(2a)and2’,5’-dide-oxyuridinylcobalamin(2b),andtwoothers,2’,5’-dideoxyadenosylcobalamin(2c),and5’-deoxy-thymidylcobalamin(2d)werepreparedbyanimprovedmethod.AllthefouranalogueswereinvestigatedbyUV-visand2D1HNMRspectroscopy.Thecomparisonsanddiscussionabouttheirspectroscopicpropertiesweredone.

  • 标签: COENZYME B12 analogues COBALAMIN 2’-deoxynucleoside UV-VIS
  • 简介:Thegeometricalstructuresof2-(2-hydroxyphenyl)pyridine(PP)anditsprotonationstateswereoptimizedbymeansoftheB3LYP/6-31G(d)method.Foralltheselectedsystems,theexistenceofH-bondisinfavorofthestabilityofthesystems.Onthebasisoftheoptimizedgeometricalstructures,theirelectronicspectrumpropertieswerestudiedbytime-dependentdensityfunctionaltheory(TD-DFT)methosdviaahybridfunctionofB3LYPand6-31G(d)basisset.TheTD-DFTcalculationresultpredictstheabsorptionspectrumofPPat324nm(3.82eV),whichisinverygoodagreementwiththeexperimentalvalueof322nm(3.85eV)determinedinsolventchloroform.TheabsorptionspectraofthetwoprotonationstatesbothexertaredshiftinvariouspHmedia.

  • 标签: 理论研究 电子光谱 密度 2-(2-羟苯基)嘧啶 光谱性质
  • 简介:用密度泛函方法「BLYP/6-311G(d)」研究了SiP分子的各种可能异构体的结构、能量和红外光谱。结果表明:Si分子有5个稳定的异构体,能量最低的异构体为具有P-P桥键湖蝶形结构,其次为具有Si-Si桥键的菱形结构,而具有Si-Si中心键的直线结构能量高,并进一步将Si和C分子结构和能量上的差异进行了比较和分析。

  • 标签: 结构 光谱 磷化硅 密度泛函 能量
  • 简介:Twonovelcyclotriphosphazenederivativescontaining6-(4-hydroxyphenyl)-2,2'-bipyridine(hopbp)sidegroups,N_3P_3(dobp)_2(hopbp)_2(1)andN_3P_3(dobp)(hopbp)_4(2)(dobp=2,2'-dioxybiphenyl),weresynthesizedandcharacterized.Thesecompoundsdisplaystrongfluorescentemissionbothinsolutionandinsolidstate.Theirabsorptionandemissionspectraaresensitivetoproton:theadditionofHBF4tothemethanolanddichloromethanesolution(9∶1,volumeratio)ofcompound1ledtoared-shiftfrom350to460nmfortheemissionspectrum,andtheprocesswasalsocharacterizedbyisosbesticpointsofabsorptionspectraat267,287and313nm.

  • 标签: 二嘧啶 合成 质子 光谱学
  • 简介:Apracticalprotocoltoobtain1,1'-binaphthyl-2,2'-diaminewasdevelopedfrom2-naphtholand2-naphthylhydrazineundermildconditions:solvent-free,125-130℃,atmosphericpressure.Theconvenientproceduremakestheprocessamenableforlarge-scalesynthesisoftheversatilecompound.

  • 标签: 联萘 合成 萘酚 压下 氨基 功能化合物
  • 简介:Amildandrapidmethodwasfoundforthereductivecleavageofthecarbon-sulfurbondinthealkylthiocyanatesbysamarium/Cp2TiC12systemtogivethecorrespondingdialkyldisulfidesinmoderatetogoodyields.

  • 标签: 二烷基二硫化物 硫磺 结合剂 缩氨酸